氢化物发生电感耦合等离子体发射光谱法测定钢中微量砷

该文研究氢化物发生-电感耦合等离子体发射光谱法测定非合金钢(碳素钢)和低合金钢中微量砷的分析方法,考察高频功率、雾化压力、辅助气流量、泵速等仪器工作条件与消解用酸及用量、硼氢化钠浓度对光谱强度的影响,并讨论王水、铁基体、共存离子对测定结果的背景干扰与消除方法.确定的最佳工作条件为:高频功率为1350 W,雾化压力为22...

Determination of trace arsenic in steel by hydride generation inductively coupled plasma emission spectrometry

Working conditions of the inductively coupled plasma-emission spectrometer for determination of trace arsenic in non-alloy steel(carbon steel) and low-alloy steel were optimized, such as high-frequency power, atomization pressure, auxiliary gas flow and pump speed. The effect of digestion acid, sodium borohydride, and the background interference of aqua regia, iron matrix and coexisting ions on the measurement results were studied. The optimal conditions were as follows: high-frequency power of 1 350 W, atomization pressure of 22 psi, auxiliary gas flow of 0.5 L/min, and pump speed of 100 r/min. The sample solution was prepared with 0.500 g steel sample, dissolved by 15 mL hydrochloric acid and 5 mL nitric acid. Then the solution, containing thiourea-ascorbic acid mixed solution, and sodium borohydride solution(2%) were introduced into hydride generator and inductively coupled plasma emission spectrometer to be measured, with the analysis line of As 189.04 nm. The matrix matching method was used to eliminate background interference,and a calibration curve was established with a series of iron matrix solutions. The linear correlation was 0.999.The limit of quantification was 0.000 12%. Synthetic samples and standard samples were determined, and the results were consistent with the theoretical or certified values.